Composition for cleansing sugar and process of making same.



To all whom it may concern:

XF; 799v876 UNITED s'ra'rns eierence IIJATENT OFFICE.

CLAUS A. SPRECKELS AND CHARLES A. KERN, OF NEW YORK, N. Y. ASSIGNORS TOFEDERAL SUGAR REFlNING COMPANY, JERSEY ()iiY, NE r JERSEY, A CORPCR-ATION OF NEW JERSEY.

COMPOSITION FOR CLEANSlNG SUGAR AND PROCESS OF MAKING SAlill-l.-

Be it known that we, (inane; A. Srnncuuns and CHARLES A. KERN, citizensof the United States, and residents of the hon nigh of Manhatt-an, cityand State of New York, have in vented certain new and usefulImprovements in (Joinppsitions for (IleansinrrSugar and Processes ofMaking Same, of which the ioilowing is a full and. true description.

The object of this invention is'to produce a composition which whenmixed with sugar,

sugar-liquor, or sugar-bearing iuatcrialwill so thoroughly combinewith-and act upon the impurities contained in the material treated as toabsorb out and carry with it when removed from the treated, mass nearlyall of said impurities withou-t injuriously affecting the sugar.

In ,our Patent No. 695,150, dated April 22,

' 1902, wehave described and claimed generic ally the process ofpurifying sugar or sugar solutionsf r th employment of lllfmjuttld.

. As an example of the way in which sui fonated or sulfo oleagiuouscleansing or puriffying liquids may be prepared for use we have statedin our said patent as follows:

\Ve mix sulfuric acid, preferably of 1.835

' specific gravity, ((56 liaunu'g) or aniixturc of acids containingsulfuric acid in the proportion of, say, lifty parts, by weight. of acidwith one hundred parts, by weight, of one or more'bodies, of whichresinous bodies; fats, fatty oils, and. fatty acids and essential oilsare examples. The sulfuric acid is added to the body gradually or at allevents undcrj such conditions'tliat a low temperaturewill' bemaintained, and the mixture is allowed to.

' ess under thesecircumstances fare "as appl stand for a few hours.

Maintaining a low temperature is essential.

to the production of thc peculiar cleansing body l'i'crcin clauncd, t'orii the bodywas ox dized, as by the use of'a strong or lumin'g acid or ahigh temperature was allowcd,-a

tarry body or pasty mass would .be produced,

which would not have the required allinity or absorbent property forsugar impurities.

Specification of Letters Patent. Application filed November 19, 1901.Serial No. 82.825

we proceed as follows: Add water about-e ual, to the amountof oil vinthe orlginal mixture 10 Patented Sis pt. 19, 1905.

- Any excess of acid is removed'or neutralized either by the addition ofan alkali or by the addition of water and gravital separation. 5:, Theproportion and strength of acid above suggested may be used insulfo'nating each and every one of the substances hereinafter mentioned;but in the case of essential oils, such as turpentine, it will. bepreferable to considerably increase the .proportion'of, the oil to thesulfuric acid, even to the extent of doubling the same or more. Theproportion and strength of acid may of coursebe varied inwell-knownways, it being borne in mind that the result is that thebodiifiiihen acted upon by the 'sulfuricracid and iti' the conditionin,which it is. to beifused.will not:

contain sulfuric acid inany amount injurious. to the sugari'and willhaveau afiinity orab" 7'6 sorbent property for the-impurities, includ- Ising invert s"ugar; .gre'ater; tlianithe-adherence of such impurities toth fs'u'gar itself.

,.JlihenaQQQQQaIQinoBLBmJLeredoinmend to proceed asfollowszxlaketwoparts of a resinous body, resin-oil being an example, and add whilestirring the oil one part of sulfuric acid, preferably mixing the acid,with th'e'oil gradualiy and at all events under such conditions that alow temperature 'will v be maintained. After the incorporationof theacid allow the mixture to stand r a few hours and then preferably removeor'neutral ize the excess of acid in the mixture. f-iForif' this purposewe may neutralize the mix'tu'r by the addition of an alkali or mixtureof 'al I kalies, preferably carbonate of soda, caustic soda, carbonateot' potash, caustic potash, or; mixtures thereof. The additionof alkalit0;;-;

the sulfo'nz'tted product may be in quantity. 99 I sufiicient toneutralize only the'free sulfuricJ acid remaining, the acid being;injurious to sugar, or it may be in such quantity to'cotn plete lyneutralize also the 'sul-fonic acids. {Ifhe salts of tlie-s'ulfonic acidformedbyoun proc cable for our purposeas the acids themselv, When notneutralizing by the use -of;al-kali and mix thoroughly. On standing themixture separates into two layers, the u per: fluid; layer-being thematerial in course of treat-' ment and the lower consisting'of watercou-UUCU g [100m mixture ispractically free from water or from v with aconsiderable proportion of hydrocararts. 7 These characteristics areaflinityor ab designation of fsult'o roleaginous cleansing taining thesurplus acid and other useless products, and we leave-the mixturestanding for several hoursin a vessel properly ar' ranged and then drawoff the water containing superfluous acid, 820. To the mixture obtainedby the addition of alkalies', as above described, or by the addition ofwater, as

excess of alkali when used, we may add thereto kerosene-oil orpetroleum-oil or other hy'd rocarbon oil or a mixture containinghydrocarbon'oilj. The said sulfonated body is soluble in am-yl and ethylalcohols and'in hydrocarbon-oils, especially kerosene-oils.

A cleansing or defecating liquor of the character hereinbefore specifiedand mixed bon oil or hydrocarbon-oil mixture intimately combined with abody-sulfonated at a low temperature has distinct characteristics andproperties for the purpose of defecating or cleansing sugar and is also,so far as we have been-able to learn, a composition new in thesorbentproperty for sugar impurities-such asinvert sugar, caramel, andsaltssuperior to the adherence of such impurities to sugar itself; freedomfrom-sulfuric acid in an amount injurious tothe sugar; the body is notoxidized, owing to'maintaining a low temperature in its production; andit mixes readily with hydrocarbon oil, such as petroleum-oils.

/Vhen employing alkali to neutralize an acid, we have obtained goodresults by employing one part of caustic soda to each fifteen parts ofthe modified mixture. We have obtained good results by adding aboutfifty per cent. of kerosene-oil; but we do not state this as a fixedpercentage, since it may be materially varied.

The'use of an alkali above described for the purpose of neutralizingfree sulfuric acid in the sulfo-oleaginousbody may result, as is wellunderstood, in the production of sulfpnicacid salts in the product; butsuch salts so made are included by us under the general or defecatingliquids.

The following are bodies which .we have tested and found to act in themanner described, vizz' colophonium, (rosiri) rosin-oil, olive-oil,castor-oil, vcotton-seed oil; cocoanutoil, linseed-oil, rape-oil,peanut-oil, lard, tallow, cod-liver oil, fish-oil, (Menhaden-oiL)lard-oil, oleic acid, stearic acid, palmitic acid, butyric acid,'01l ofturpentine; but the substances above named are given as examples said,but also defecating or cleansing liquids containing sulfo-oleaginousbodies made by the subjection of mixtures of two or more of suchresinous, fatty, or oily bodies to the action of sulfiiric'acid. We haveobtained good results from a considerable number of such mixtures, ofwhich the following may be cited as examples: first, rosin-oil,castor-oil, and oleic acid: second,- castor-oil, cotton-seed oil, andole'icacid; third, lard and rosinoil; fourth, rosin-oil, oleicaid, andoilof turpentine; fifth, tallow and oil of turpentine.

As most of the above-enumerated .bodies are known as oils and as rosinis analogous to fatty bodies for the purposes of our invention and asthe fats are solid oils and as the fatty acids, as is well known, haveoily or greasy characteristics and as all of the above substances areacted upon by sulfuric acid in the manner described and also whensulfated act on sugar and its impurities in analogous and equivalentways, we hereinafter include them all under the generic term-oleaginousbodies, and when acted on by sulfuricacid in the manner described weterm the derivatives sulfo-oleaginous bodies. All the derivativecleansing agents mentioned are properly included-also under the termsulfonated bodies whether properly and strictly called olea ginous ornot. Many'forms of wifeoleaginons bodies, especially sulfonic acids orsulfonic-acid bodies,are well known in the arts for other purposes, andhence a more particu-.

lar description ofthe methods-of producing the same is not required.

In preparing the sulfonated fluid defecating or cleansing agentconstituting the subject-matterof our claims the hydrocarbon oil ormixture of hydrocarbon oil may sometimes be added before or sometimesafter subjecting the'bodies hereinbeforc specified tothe action of theacid or acid mixture. For

tion of kerosene-oil. 7 z

foo

finstance, bodies containing palmitic acid, stearic acid, butyric acidor rosin may be first softened or rendered fluid by the addi-' differentqualities .of the material being treated, enough beingused, of course,to absorb out. the impurities. As the liquid has no injuriousefiect'upon the sugar, sugarliquor, or sugar-bearing material, thequantity of theliquid may be increased as desired. The mixture orcombination of sulfonated fluid defecating or cleansing agent with sugar232. UUlVHUol l lunlo.

' defecating liquid are described and claimed 7 cross produces anintermediate product, which constitutes the subject-matter of LettersPatent of the United States No. 703,219, granted June 24, 1902, to us.

Methods of treatment of sugaror sugar solution by the use of our newcleansing or generically in United States Letters Patent No. 698,150,granted April 22, 1902, to us, and as to dilferent specific methods inUnited States Letters Patent No. 699,933, granted to us May 13, 1902,and in United States Letters Patent No. 700,099, granted to us May Wehave described and claimed in-a subordinate patent granted March 3,1903, as No.

' 722,157, sulfonated fluid defecatingofcleansing agents made bytreating ditferent groups and special bodies which we have foundefiicient in producing the desired result.

We desire it clearly understood that while we'specify sulfonateddefecating or cleansing liquids, made by treating certain substances ormixtures as described, yet our in vvention herein claimed is not limitedto the substances and mixtures specifically mentioned nor to anyspecific way of removin excess of acid or free acid.

We claim-'- 1. As a'new article of manufacture, a sugarcleansingcompound, consisting of a solution in hydrocarbon oil of a sulfonatedderivative 'of a resinous body, which derivative is soluble in ethyl andamyl alcohols, substantially as described.

2. As anew article of manufacture, a sugar' cleansing compoundconsisting of a solution in kerosene-oil of a sulfonated derivative of aresinous body, substantially as described.

As a new article of manufacture, a sugarcleansing compound consisting ofa solution in hydrocarbon oil of asulfonated body soluble in ethyl andamyl alcohols, substantially as. described.

\ Q 4. As a new article of manufacture, a sugarcleansing compoundconsisting of a solution in hydrocarbon oil of a sulfonated derivativeof an oljeaginous body, which derivative is solublein ethyl and amylalcohols, substan-. tially as described. 1

5. As a new article of manufacture, a sugarcleansing compound consistingof a solution in hydrocarbon oil of a'sulfonated derivative ofrosin-oil, whichderivative, is soluble in ethyl and amyl alcohols,substantially as described. 1

6. As a new article of manufacture, a sugarcleansing compound consistingof a solution in kerosene-oil of asulfonated body, substantially asdescribed.

7. As a new article of manufacture, a sugarcleansing compound consistingof a solution in keroseneoilof a sulfonated derivative of an oleaginousbody,.substantially as described.

8. As a new article of manufacture, a sugarcleansing compound consistingof a solution in kerosene-oil of a sulfonated derivative of rosin-oil,substantially as described;

9. The process of making a sugar-cleansing compound which consists inproducing a sulfrom the'mixture, and then adding keroseneoil to theseparated sulfonated body, substantially as described. 4

'11. The process of making-a sugar-cleansing compound'which consists inmixing a resinous body with sulfuric acid, while a low tem: perature ismaintained, then completely separating resulting sulfonated body fromthe mixture, and then adding hydrocarbon oil to pletely separatingresulting sulfonated body the separated sulfonated body, substantiallyas described.

12. The process of making a sugar-cleansing compound which consists inmixing rosinoil with sulfuric acid, while a low temperature ismaintained, then completely separating resulting sulfonated body fromthe mixture, and then adding kerosene-oil to the separated sulfonatedbody, substantially as described.

CLAUS A. sPREcKELs.

I CHARLES A. KERN .Witnesses: WILLIAM W. Oo'ox, ,WrLLIAM H. BE'BRIGAN,Jr.

